Microplastics persist in wastewater treatment plant (WWTP) effluents despite high overall inherent removal efficiencies, primarily due to their colloidal stability and resistance to gravitational settling. This study integrates field-scale profiling with mechanistic investigations to elucidate how charge-regulated interactions influence microplastic aggregation and removal. Using laser infrared imaging, we quantify the abundance, composition, and morphology of microplastics across multiple WWTPs and reveal a persistent fraction of sub-250 µm particles in treated effluents. To clarify the underlying physicochemical mechanisms, model polystyrene nanoplastics are treated with a cationic metal-organic complex to induce aggregation. Dynamic light scattering and zeta potential measurements indicate a non-monotonic, re-entrant transition from dispersion to aggregation, followed by re-stabilization, governed by charge neutralization and inversion. Small-angle neutron scattering reveals the formation of surface-fractal aggregates near charge neutrality, linking interparticle interactions to mesoscale structure. Based on this mechanistic framework, targeted charge compensation in real wastewater has been shown to induce rapid aggregation and facilitate the removal of up to 90% of residual microplastics, resulting in an overall removal efficiency approaching 99%. Our findings establish charge-regulated aggregation as a strategy to overcome colloidal stability in microplastic-laden effluents and provide a physicochemical foundation for improving existing wastewater treatment processes.

The cooperative gelation of sPS with the short PEGDME molecules (molecular weight MW = 1.5 kg mol-1) from a common THF solution is driven by the gelation tendency of sPS at a temperature around 40 degrees C. The crystalline junctions in the wet gel are fibrillar morphologies, which are typically composed of sPS and PEG molecules, as shown by contrast variation SANS, and consist of sPS, which co-crystallizes in d-form with the solvent molecules, and to a certain extent with PEGDME molecules, as demonstrated by the conformational change of both polymer types from an amorphous to a helical form when the gelation temperature is exceeded, which was observed by in situ FTIR. XRD and SEM on drying gels have shown that the large-scale morphology of dry gels, when the polymer strands collapse and crystalline polymer strands are formed, is determined by the presence and length of the PEGDME molecules. While the sPS dry gel exhibits a more homogeneous distribution of polymer strands and well-defined pores, the polymer strands of the gel with short PEGDME connect at one end to form "tufted" macroassemblies, which, due to the additional co-crystallization of PEGDME with sPS, leads to very large pores and voids.

Hybrid implants consisting of a permanent Ti-based part combined with a degradable Mg part, are promising solutions to design superior implants by combining the advantages of both materials.

This study investigates the impact of silicon content in the graphite anode of cylinder-type Li-ion batteries using operando neutron powder diffraction techniques. A batch of four different Li-ion cells is analyzed, with a focus on the structural response of active cell components during electrochemical cycling. The results indicate that high silicon content in the graphite anode causes a delay in the initial lithiation of graphite, shifting it towards higher voltages independent of the cell's internal resistance. Differential voltage, incremental capacity analyses and quantitative energy-dispersive X-ray spectroscopy, corroborate these structural changes. Additionally, X-ray diffraction computed tomography using a mu m-sized synchrotron beam revealed local structural degradation and lithiation inhomogeneity in the high silicon content cells during cycling.

In this contribution, we report the synthesis of a poly(4-vinylpyridine)-reduced graphene oxide-magnetite (P4VP-rGO-Fe₃O₄) organo-magnetogel (OMG), designed for high-performance pollutant adsorption. In the OMG, rGO and Fe₃O₄ nanoparticles are in situ encapsulated during the chemical cross-linking of the 4-vinylpyridine polymer. The adsorption performance of OMG was evaluated using three model water pollutants, viz., organic dyes, heavy metal ions, and waterborne pathogens. The equilibrium adsorption capacity exceeded 400 mg/g for the organic dyes. Beyond dye removal, the OMG also adsorbed heavy metal ions, such as AsO2−, Pb²⁺, Cr2O72−, and Cd²⁺ ions, with removal efficiencies exceeding 60% and adsorption capacities exceeding 200 mg/g. The OMG also exhibited remarkable antibacterial activity against E. coli and S. Typhi, with almost zero viability for S. Typhi. The OMG promises a broad-spectrum applicability in wastewater treatment, offering a sustainable and efficient solution for water decontamination.

Structural and spatial aspects of cell degradation are studied using a combination of diffraction-and imaging-based tools applying laboratory X-rays, neutron scattering and synchrotron radiation with electrochemical and thermal characterization. Experimental characterization is carried out on cylindrical cells of 21700-type, where four regimes of cell degradation are identified, which are supplemented by an increased cell resistance and surface temperature during cell operation. The amount of intercalated lithium in the fully charged anodes in the fresh and aged states is determined by ex situ X-ray diffraction radiography and in situ X-ray diffraction computed tomography. The qualitatively similar character of the results revealed a loss of active lithium along with the development of a complex heterogeneous distribution over the electrode stripe.

A full series of variously lithiated graphite anodes material LixC6 (0<x<1) corresponding to a different state-of-charge (SOC) between 0 % and 100 % was collected from 18650-type cylinder Li-ion batteries, and the thermal structural behavior of these electrodes was mapped using ex situ high-resolution X-ray and neutron diffraction. Their structural behavior was analyzed over a broad temperature range. At high temperatures, a non-reversible decomposition of the lithiated graphite anodes takes place, accompanied by a loss of intercalated lithium ions, forming novel phases such as LiF and Li2O strongly coupled to the degradation of the solid electrolyte interface (SEI). Complementary calorimetric measurements showed the strongly exothermic chemical reactions during the decomposition matching well to the collected diffraction data. Post mortem analysis applying scanning electron microscopy revealed various morphological features supplementing the treatment of battery anodes and highlighted the importance of the SEI layer during the cycling of the cell and its thermal degradation.

The additively manufactured AlSi10Mg alloy demonstrates considerable residual stresses, adversely affecting the dimensional accuracy, operational safety, and corrosion resistance of the parts. In practical applications, stress relief annealing is necessary to eliminate residual stresses in residual stresssensitive applications. However, the current understanding of the mechanical properties of the additively manufactured AlSi10Mg alloy after annealing is still limited to the macroscopic level. To further investigate the micromechanical behavior and intrinsic mechanisms of the alloy, this study employed synchrotron Xray diffraction technology to conduct in situ deformation analysis. This study thoroughly examined the lattice strain and stress evolutions of the Al and Si phases and clarified the individual contribution of each phase to the strain hardening rate of the alloy. In addition, this study quantitatively assessed the evolution of dislocation density and elucidated the influences of annealing heat treatment on the load transfer and dislocation behavior of the additively manufactured AlSi10Mg alloy.

The dissolution of nano-sized Ni3Al-based γ′ precipitates was investigated in the newly developed polycrystalline nickel-based VDM® Alloy 780 at the surface and in the bulk region with in-situ lab-source and synchrotron X-ray diffraction. These studies are important in obtaining a deeper understanding of the strengthening mechanism responsible for the stability and long service lives of such superalloys. We found that the dissolution behavior of the γ′ phase is very similar at the surface and in the bulk region, but small deviations were detected. The dissolution of γ′ starts at around 800 °C and no γ′ was found at temperatures exceeding 970 °C. As a result, the elements Al and Nb, which were bound in the γ′ phase, dissolved into the γ matrix and strongly increased the γ lattice parameter, as their atomic size is larger than the γ-forming elements Ni, Co, and Cr. However, this effect was suppressed in the surface area. A second matrix γ phase was detected at the same temperature range as that of the dissolution of the γ′ phase in the lab-source XRD measurements. The newly formed γ-2 phase had a smaller lattice parameter than that of the initial γ matrix. We propose that the γ-2 matrix phase is a result of high-temperature surface oxidation, which consumes, among other elements, Al and Nb and, therefore, leads to the smaller γ lattice parameter.

The morphology and ionic conductivity of a high-molecular-weight polystyrene-block-poly(ethylene oxide) (PS-b-PEO) diblock copolymer (DBC) solid-state hybrid electrolyte, prepared entirely from solution, containing the lithium salt LiTFSI ([Li]/[EO] = 0.1) and titania (TiO2) nanoparticles (NP) were investigated at different temperatures. Structure investigation using small-angle X-ray scattering (SAXS) indicates a rupture of the DBC morphology upon increasing TiO2-NP content, without a significant decrease in the ionic conductivity at high TiO2-NP contents. A high number of unbound charge carriers in the hybrid DBC electrolyte, achieved by careful tuning of the materials' ratios, is the most important contribution to a high ionic conductivity.

In the field of magnetoelectric coupling, especially via the spin-dependent metal–ligand d-p hybridization mechanism found in multiferroic Ba 2 ${M}$ Ge 2 O 7 ( ${M}$ = Mn, Co), detailed knowledge of the microscopic structural parameters is essential, also for the theoretical modeling. In this article, we report a systematic structural study of Ba 2 MnGe 2 O 7 single crystal under varying temperatures between 110 and 673 K using non-destructive in situ single crystal synchrotron radiation diffraction. The maximum entropy method (MEM) was applied to the X-ray diffraction data for the determination of the deformation in the electron density and the orbital hybridization between the 3d of Mn and 2p of O in the Mn–O bond. Within this entire temperature range, the structure was described in a single crystallographic space group $P\bar {4}2_{1}m$ and no structural phase transition has been detected. Interestingly, the forbidden reflections, which arise from multiple diffractions so-called “Renninger effect,” were observed at all temperatures without any symmetry lowering. The changes in the structural parameters [bond-lengths, bond-angles, anisotropic displacement parameters, and electron density distributions (EDDs) of the atoms] with temperature are revealed, helping to understand some aspects comprising orbital hybridization in multiferroic Ba 2 MnGe 2 O 7 .

Physical properties of nanoclusters, nanostructures and self-assembled nanodots, which in turn are concomitantly dependent upon the morphological properties, can be modulated for functional purposes. Here, in this article, magnetic nanodots of Fe on semiconductor TiO 2 nanotubes (TNTs) are investigated with time-of-flight grazing incidence small-angle neutron scattering (TOF-GISANS) as a function of wavelength, chosen from a set of three TNT templates with different correlation lengths. The results are found corroborating with the localized scanning electron microscopy (SEM) images. As we probe the inside and the near-surface region of the Fe-dotted TNTs with respect to their homogeneity, surface distortion and long-range order using TOF-GISANS, gradual aberrations at the top of the near-surface region are identified. Magnetization measurements as a function of temperature and field do not show a typical ferromagnetic behavior but rather a supermagnetic one that is expected from a nonhomogeneous distribution of Fe–dots in the intertubular crevasses.

Efficient infiltration of a mesoporous titania matrix with conducting organic polymers or small molecules is one key challenge to overcome for hybrid photovoltaic devices. A quantitative analysis of the backfilling efficiency with time-of-flight grazing incidence small-angle neutron scattering (ToF-GISANS) and scanning electron microscopy (SEM) measurements is presented. Differences in the morphology due to the backfilling of mesoporous titania thin films are compared for the macromolecule poly[4,8-bis-(5-(2-ethyl-hexyl)-thio-phen-2-yl)benzo[1,2-b;4,5-b']di-thio-phene-2,6-diyl-alt-(4-(2-ethyl-hexyl)-3-fluoro-thieno[3,4-b]thio-phene-)-2-carboxyl-ate-2-6-diyl)] (PTB7-Th) and the heavy-element containing small molecule 2-pinacol-boronate-3-phenyl-phen-anthro[9,10-b]telluro-phene (PhenTe-BPinPh). Hence, a 1.7 times higher backfilling efficiency of almost 70% is achieved for the small molecule PhenTe-BPinPh compared with the polymer PTB7-Th despite sharing the same volumetric mass density. The precise characterization of structural changes due to backfilling reveals that the volumetric density of backfilled materials plays a minor role in obtaining good backfilling efficiencies and interfaces with large surface contact.

The most daunting challenge in solid-state polymer electrolyte membranes (PEMs) is to achieve high ionic conductivity close to that of the liquid electrolytes, while maintaining enhanced thermal and mechanical performances. The ionic conductivity in relation to the morphology of PEMs composed of diblock copolymer (polystyrene-block-poly(ethylene oxide); PSb-PEO), lithium salt (lithium trifluoromethanesulfonate; LiTO, and ionic liquid (1-ethyl-3-methylimidazolium trifluoromethanesulfonate; EMIMTf) is investigated. The optimized functional nanostructured PEMs are achieved with room-temperature ionic conductivities higher than a 1 mS cm(-1) benchmark. The morphology of these microphase-separated electrolytes is composed of a major soft high ionic-conductive PEO/LiTUIL matrix with minor glassy high-modulus PS nanodomains. The ionic-liquid upload in hybrid electrolytes inhibits the PEO crystallization, reduces the PEO glass transition temperature, promotes an extended PEO chain conformation, and enhances the solubilization of the non-dissociated lithium salt at the PS-PEO domain interfaces. These intrinsic properties caused by the ionic-liquid loading serve to achieve stable and robust nanostructured electrolyte membranes and can explain the achieved benchmark conductivity.

Na-ion batteries have recently attracted great attention regarding their application in large-scale energy storage systems. Among different types of electrode materials for those classes of batteries, so-called Prussian blue analogues (PBAs) are among the very attractive ones due to their comparatively simple and low-cost methods of synthesis coupled with a promising cycle performance. In this study, one of the state-of-the-art PBA battery materials, namely electrodeposited Na2Ni[Fe(CN)(6)] (NiHCF) thin films, were tested under simulated battery conditions in aqueous and mixed (H2O/organic) electrolytes. Prolonged stability tests in aqueous electrolytes were performed together with in-operando electrochemical AFM monitoring. It is demonstrated that degradation of this material is not associated with noticeable morphological changes (mechanical stress) but is likely caused by changes in the chemical composition of the films. Intercalation and deintercalation reversibility of Na+ and thin film stability in aqueous electrolytes appear to be unaffected negatively by changes in the pH to values below 7. However, the films showed unstable behavior in basic media (pH > 10). The increase of the content of acetonitrile, which was used as an additive to simulate the influence of antifreezes in aqueous electrolytes, appears to primarily affect the deintercalation of Na ions in Na2SO4-based aqueous electrolytes.

The effect of the addition of n-hexanol as co-surfactant on the structure of cetyltrimethylammonium bromide (CTAB) micelles has been studied using small-angle X-ray and neutron scattering (SAXS, SANS). Contrast variation neutron scattering experiments were performed to determine the structure of both pure CTAB and n-hexanol modified CTAB micelles. The incorporation of n-hexanol leads to an elongation of the ellipsoidal CTAB micelles. The scattering length density of the micellar shell linearly depends on the degree of deuteration of the dispersion medium water and revealed the existence of substantial amounts of water in the micellar shell. The water content in the shell increased from 20 vol-% observed for pure CTAB micelles to 44 vol-% found for n-hexanol modified CTAB micelles. The amount of n-hexanol in the micellar shell was determined by varying the amount of fully deuterated and protonated n-hexanol. These experiments revealed a volume fraction of 26 vol-% of n-hexanol molecules in the micellar core which equals a molar fraction of 50 % n-hexanol within the CTAB micelles. The total composition of micellar core and shell was estimated. The packing density of headgroups, water molecules and bromide ions turned out to drastically increase in n-hexanol modified CTAB micelles. These findings contribute to a fundamental understanding of the stabilization mechanism of micelles by alcoholic co-surfactants and the resulting alteration of the morphology and interface composition. These results will facilitate the optimization of processes where CTAB and other comparable surfactants are used as phase transfer catalysts, structure directing agents or stabilizers in colloidal dispersions or emulsions.

ZnO nanoparticles (NPs) are highly relevant for various industrial applications, however, after synthesis of the NPs residual chemicals need to be removed from the colloidal raw product by washing, as they may influence the performance of the final device. In the present study we focus on the effect of washing by antisolvent flocculation with subsequent redispersion of the NPs on the stabilizing acetate shell. Purification of the ZnO nanoparticles is reported to be optimal with respect to zeta potential that has a maximum after one washing cycle. In this work, we will shed light on this observation using small angle X-ray and neutron scattering (SAXS, SANS) by demonstrating that after the first washing cycle the content of acetate in the ligand shell around the ZnO NPs increases. In detail, it was observed that the diffuse acetate shell shrinks to the size of a monolayer upon washing but the acetate content of this monolayer is higher than within the diffuse shell of the particles of the native dispersion. A second washing cycle reduces the acetate concentration within the stabilizing shell and the stability of the dispersion drops accordingly. After another (third) washing cycle strong agglomeration was observed for all investigated samples.

The analysis of lithium-ion battery aging relies on correct differentiation between irreversible and reversible capacity changes. Anode overhang regions have been observed to influence Coulombic Efficiency (CE) measurements through lithium diffusion into and out of these areas, complicating precise capacity determination. This work presents an analysis of the extent of graphite anode overhang lithiation after calendar storage by means of local X-ray diffraction (XRD), CE measurements, and color change analysis. We found LiC12 lithiation of the anode overhang area after 20 month storage at 40 degrees C at high state of charge (SoC) and partial lithiation (LiC18) at medium SoC storage at 40 degrees C and 25 degrees C. Graphite color changes in the overhang areas are observed and consistent with the state of lithiation measured by XRD. Coulombic efficiencies greater than unity and increasing capacity during 1200 h of cycling are detected for high SoC storage cells. The capacity difference between high and low storage SoC batteries decreases by up to 40 mAh (3.6% of nominal capacity) after cycling compared to tests directly after storage. Consequently, the size of the anode overhang areas as well as the battery storage temperature and duration need to be considered in CE analysis and state of health assessment. (C) 2017 Elsevier B.V. All rights reserved.

Rotary friction welding (RFW) was used in the current study to join the dissimilar metals AA7020-T6 aluminium alloy and 316L steel. Neutron diffraction was performed to investigate the texture gradient around the weld line and to map the residual stress over the whole specimen. The texture analysis showed a weak shear component near the bond line of AA7020-T6-T6 side which indicated a plastic deformation of AA7020-T6 during welding. The shear bands were also observed in optical microstructures. Relatively high tensile residual stresses were observed near the bond line on the AA7020-T6 side, which were in-homogeneously distributed from the perimeter to the rod centre, while high compressive residual stresses were found in the sample centre at the bond line in the 316L steel.